Nitrite DOC316.53.

01178

Ceric Acid Titration Method Method 8351

100–2500 mg/L as NaNO2 Digital Titrator
Scope and application: For cooling tower waters.

Test preparation

Before starting
The optional TitraStir Titration Stand can hold the Digital Titrator and stir the sample.
Review the Safety Data Sheets (MSDS/SDS) for the chemicals that are used. Use the recommended personal protective
equipment.
Dispose of reacted solutions according to local, state and federal regulations. Refer to the Safety Data Sheets for disposal
information for unused reagents. Refer to the environmental, health and safety staff for your facility and/or local regulatory
agencies for further disposal information.

Items to collect
Description Quantity

Ferroin Indicator Solution 1

Sulfuric Acid Standard Solution, 5.25 N 1
Ceric Standard Solution Titration Cartridge, 0.5 N 1
Digital Titrator 1
Delivery tube for Digital Titrator 1
Graduated cylinder (use a size that is applicable to the selected sample volume) 1
Erlenmeyer flask, 125 mL 1
Water, deionized varies

Refer to Consumables and replacement items on page 4 for order information.

Sample collection and storage

• Collect samples in clean glass or plastic bottles.
• Analyze the samples as soon as possible for best results.
• If immediate analysis is not possible, keep the samples at or below 6 °C (43 °F) for a
maximum of 24 hours.
• Let the sample temperature increase to room temperature before analysis.

1
Test procedure
1. Select a sample volume
from Table 1 on page 3.
5. Pour the sample into a
clean, 125-mL Erlenmeyer
flask.
9. Add one drop of Ferroin
Indicator Solution.
1 A pipet is recommended for sample volumes less than 10 mL.
2 Nitrite, Ceric Acid Titration—Digital Titrator (2500 mg/L)
2. Insert a clean delivery
tube into the digital titration
cartridge. Attach the
cartridge to the Digital
Titrator.
6. Dilute to approximately
75 mL with deionized water.
10. Swirl to mix.
3. Hold the Digital Titrator 4. Use a graduated cylinder
with the cartridge tip up. or a pipet1 to measure the
Turn the delivery knob to sample volume from Table 1
eject air and a few drops of on page 3.
titrant. Reset the counter to
zero and clean the tip.
7. Add 5 drops of 5.25 N 8. Swirl to mix.
Sulfuric Acid Standard
Solution.
11. Put the end of the 12. Use the multiplier in
delivery tube fully into the Table 1 on page 3 to
solution. Swirl the flask. calculate the concentration.
Turn the knob on the Digital Digits used × digit multiplier
Titrator to add titrant to the = mg/L sodium nitrite as
solution. Continue to swirl NaNO2.
the flask. Add titrant until the
color changes from orange
to pale blue. Record the
number of digits on the
counter.
Sample volumes and digit multipliers
Select a range in Table 1, then read across the table row to find the applicable
information for this test. Use the digit multiplier to calculate the concentration in the test
procedure.
Example: A 25-mL sample was titrated with 0.5 N Ceric Standard Solution Titration
Cartridge and the counter showed 250 digits at the endpoint. The concentration is
250 digits x 0.86 = 215 mg/L sodium nitrite as NaNO2.
Table 1 Sample volumes and digit multipliers
Range (mg/L as NaNO2) Sample volume (mL) Digit multiplier
100–400 25 0.86
400–800 10 2.15
800–1500 5 4.31
1500–2500 2 10.78

Accuracy check
Standard solution method
Use the standard solution method to validate the test procedure, reagents, apparatus and
technique.
Items to collect:
• Sodium Nitrite, ACS
• 1000-mL volumetric flask, Class A
• 5-mL volumetric pipet, Class A and pipet filler safety bulb
• Deionized water

1. Prepare a 1000-mg/L sodium nitrite standard solution as follows:

a. Add 1.000 gram of sodium nitrite to the volumetric flask.
b. Dilute to the mark with deionized water. Mix well.
2. Use the test procedure to measure the concentration of the prepared standard
solution. Use 5.0 mL of the prepared standard solution.
3. Compare the actual result to the correct result. The correct result for this titration is
approximately 1000 mg/L as NaNO2.

Standardization of the ceric standard solution

The normality of the ceric standard solution can decrease over time. Before use, examine
the normality with the standardization procedure. It is recommended to do the
standardization procedure monthly.
Items to collect:
• Sodium Thiosulfate Titration Cartridge, 0.200 N
• 125-mL Erlenmeyer flask
• Deionized water

1. Use a graduated cylinder to measure 50 mL of deionized water into a 125-mL

Erlenmeyer flask.
2. Use a pipet to add 5 mL of 19.2 N Sulfuric Acid Standard Solution. Swirl to mix.
3. Insert a clean delivery tube into the Ceric Standard Titration Cartridge. Attach the
cartridge to the titrator.
4. Hold the Digital Titrator with the cartridge tip pointing up. Turn the delivery knob to
eject a few drops of titrant. Reset the counter to zero and wipe the tip.
5. Put the delivery tube into the solution and swirl the flask. Turn the knob on the titrator
to add 200 digits of titrant to the solution.

Nitrite, Ceric Acid Titration—Digital Titrator (2500 mg/L) 3

 6. Insert a clean delivery tube into a 0.200 N Sodium Thiosulfate Titration Cartridge.
Attach the cartridge to the titrator.
7. Hold the Digital Titrator with the cartridge tip pointed up. Turn the delivery knob to
eject a few drops of titrant. Reset the counter to zero and clean the tip.
8. Titrate the solution until the color changes from intense yellow to faint yellow. Record
the number of digits on the counter. The correct number of digits for this step is
400–450 digits.
9. Add 1 drop of Ferroin Indicator Solution to the flask. Swirl to mix. The color of the
solution changes to faint blue.
10. Continue the titration with Sodium Thiosulfate until the color changes to orange.
Record the number of digits on the counter.
11. Divide the number of digits by 500 to calculate the correction factor.
12. Multiply the mg/L sodium nitrite from the titration procedure by the correction factor to
get the correct sodium nitrite concentration.

Summary of method
Ferroin indicator and acid is added to the sample. The sample is titrated with tetravalent
cerium ion, which is a strong oxidant. After the cerium oxidizes the nitrite, the indicator is
oxidized and causes a color change from orange to pale blue. The quantity of titrant used
changes in relation to the concentration of sodium nitrite in the sample.
Consumables and replacement items
Required reagents

Description Quantity/Test Unit Item no.

Ceric Standard Solution Titration Cartridge, 0.5 N 1 each 2270701

Ferroin Indicator Solution 1 29 mL DB 181233
Sulfuric Acid Standard Solution, 5.25 N 1 100 mL MDB 244932

Required apparatus

Description Quantity/test Unit Item no.

Cylinder, graduated, 100 mL 1 each 50842

Digital Titrator 1 each 1690001
Delivery tube for Digital Titrator, J-hook tip 1 5/pkg 1720500
Flask, Erlenmeyer, 125 mL 1 each 50543
Pipet filler, safety bulb 1 each 1465100
Pipet, volumetric, Class A, 2.00 mL 1 each 1451536
Pipet, volumetric, Class A, 5.00 mL 1 each 1451537
Pipet, volumetric, Class A, 10.0 mL 1 each 1451538
Pipet, volumetric, Class A, 20.0 mL 1 each 1451520

Recommended standards

Description Unit Item no.

Sodium Nitrite, ACS 454 g 245201

Sodium Thiosulfate Titration Cartridge, 0.200 N each 2267501
Sulfuric Acid Standard Solution, 19.2 N 100 mL 203832

4 Nitrite, Ceric Acid Titration—Digital Titrator (2500 mg/L)

Optional apparatus

Description Unit Item no.

®
Ampule Breaker, 10-mL Voluette Ampules each 2196800
®
Pipet, TenSette , 1.0–10.0 mL each 1970010
®
Pipet tips for TenSette Pipet, 1.0–10.0 mL 50/pkg 2199796
Stir bar, octagonal each 2095352
TitraStir® Titration Stand, 115 VAC each 1940000
TitraStir® Titration Stand, 230 VAC each 1940010
Delivery tube for Digital Titrator, 90-degree bend for use with TitraStir Titration Stand 5/pkg 4157800

Nitrite, Ceric Acid Titration—Digital Titrator (2500 mg/L) 5

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